CN1295275C - Method for surface modification of carbon nanotube and its dispersion method in epoxy resin - Google Patents
Method for surface modification of carbon nanotube and its dispersion method in epoxy resin Download PDFInfo
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- CN1295275C CN1295275C CNB2005100097690A CN200510009769A CN1295275C CN 1295275 C CN1295275 C CN 1295275C CN B2005100097690 A CNB2005100097690 A CN B2005100097690A CN 200510009769 A CN200510009769 A CN 200510009769A CN 1295275 C CN1295275 C CN 1295275C
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Abstract
The present invention relates to a carbon nanometer tube surface modification and a dispersion method for the carbon nanometer tube surface modification in epoxy resin. The method comprises the steps: (a) a purified carbon nanometer tube with the tube diameter of 0.5 to 500 nm and the length of 200 nm to 40 mu m, coupling agents and organic solvents are mixed for reaction for 10 to 20 min in the agitation state; a certain quantity of dispersing agents and a certain quantity of organic solvents are added in the mixture which is uniformly mixed, and ultrasonic waves are used for treating for 20 to 40 min after the uniform agitation is carried out; (c) the uniform dispersion solution and a certain amount of epoxy resin are uniformly mixed at high speed for 10 to 20 min. The carbon nanometer tube in the system has the advantages of easy and uniform dispersion and stable systems.
Description
Technical field:
The present invention relates to a kind of surface modification and dispersion technology of nanotube, belong to a kind of surface modification of carbon nanotube and the dispersing method in Resins, epoxy thereof.
Background technology:
Carbon nanotube is since 1991 are found, because its exclusive structure and peculiar physics, chemical property, as the metal of uniqueness or semi-conductor electroconductibility, high physical strength, hydrogen storage ability, adsorptive power and stronger microwave absorption capacity etc., and potential application prospect and be subjected to people's attention day by day, cause various countries scientists' very big interest, become one of the international research focus in fields such as physics, chemistry, materialogy at present.Applied research shows that carbon nanotube can be used for multiple high-tech area.As with it as toughener and conductive agent manufacturability can be good automobile protective spare, make support of the catalyst with it and can significantly improve activity of such catalysts and selectivity, the microwave absorbing property that carbon nanotube is stronger makes it can be used as absorption agent and prepares stealth material, electromagnetic shielding material or darkroom absorbing material etc.
Carbon nanotube is considered to a kind of new function material and structured material of excellent performance, and all in preparation and a large amount of research and development strength of application facet input, expectation can be captured the commanding elevation of this technical field in countries in the world.But, because the carbon nanotube metal nanometer material, very easily assemble, if them as common carbon fibers and mixed with polymers, carbon nanotube is easy to be gathered into useless agglomerate, can't bring into play its high-performance.
Summary of the invention:
Very easily assemble in order to solve existing carbon nanotube, be easy to be gathered into useless agglomerate, can't bring into play the problem of its high-performance, the invention provides a kind of surface modification of carbon nanotube and the dispersing method in Resins, epoxy thereof, this method is to utilize effects such as the dispersion of ultrasonic wave and high-speed stirring decollator, pulverizing, activation, the gathering of destroying carbon nanometer tube itself and winding; Utilize the organo-functional group and the carbon nano tube surface of tensio-active agent to carry out chemisorption or chemical reaction, make tensio-active agent cover carbon nano tube surface, thereby realize surface modification of carbon nanotube and the dispersion in Resins, epoxy thereof, make carbon nanotube can not be gathered into agglomerate, give full play to its high-performance.
The technical solution adopted in the present invention is: be purified caliber 0.5-500nm (a), length is that 1-2 part carbon nanotube and the 1-2 part coupling agent of 200nm-40 μ m stirs hybrid reaction 10-20 minute in organic solvent;
(b) will add dispersion agent of 3-6 part and the organic solvent of 30-40 part in the above-mentioned mixture that mixes, after stirring, use ultrasonication 20-40 minute;
(c) with the Resins, epoxy high-speed stirring of above-mentioned finely dispersed solution and 55-60 part 10-20 minute, mix.
Aforementioned proportion all calculates by weight.
Above-mentioned said carbon fiber static-conducting coating Resins, epoxy is selected from least a among Resins, epoxy E-20, epoxy resin E-44 or the Resins, epoxy E-12; Coupling agent is at least a in silane coupling agent or the titanate coupling agent; Dispersion agent is at least a in polyacrylic ester or the modified polyurethane; Organic solvent is selected from least a in dimethylbenzene, propyl carbinol or the pimelinketone.
The invention has the beneficial effects as follows: because this surface modification of carbon nanotube and the dispersing method in Resins, epoxy thereof, be by utilizing the dispersion of ultrasonic wave and high-speed stirring decollator, pulverize, effects such as activation, carbon nano tube surface is handled, has dispersion easily with carbon nanotube in the system of the present invention's formation, evenly, system is stable and with the static conductive coating of the mixture preparation of this preparation, the electrical conductor consumption is few, excellent oil resistance, erosion resistance, thermotolerance, solvent resistance, surface drying is fast, strong adhesion, good with the metallic substance bonding force, the hardness height, wear resistance is extremely strong, stable performance, pollution-free to oil product, long service life.
Embodiment:
Present invention is described below by embodiment, and according to the carbon nano tube/epoxy resin mixed system that following technology forms, the carbon mitron is uniformly dispersed, and system is stable, easily and color stuffing and auxiliary agent be hybridly prepared into the static conductive coating of excellent performance.
Embodiment 1:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent TM-10 and 3 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 12 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,23 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Embodiment 2:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.2 gram of 200nm-40 μ m, 0.2 gram silane coupling agent TM-10 and 3 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.2 gram dispersion agent EFKA4010,0.2 gram dispersion agent DP9100 and 12 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 20 minutes, add 0.1 gram EFKA4009,0.1 gram EFKA2022,24 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Embodiment 3:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent TM-10 and 3 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 12 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 20 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,23 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Embodiment 4:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent KH-560 and 3 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 12 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,23 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Embodiment 5:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent TM-10 and 3 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 12 gram dimethylbenzene, propyl carbinol, the pimelinketone mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,23 gram epoxy resin E-44 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperse evenly especially, system is stable.
Embodiment 6:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent KH-560 and 3 gram dimethylbenzene, propyl carbinol, the cyclohexanone mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 12 gram dimethylbenzene, propyl carbinol, the cyclohexanone mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,23 gram epoxy resin E-44 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperse evenly especially, system is stable.
Embodiment 7:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent TM-10 and 2 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 5 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,11 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Embodiment 8:
Is purified average caliber 0.5-500nm, length is carbon nanotube 0.4 gram of 200nm-40 μ m, 0.4 gram silane coupling agent KH-560 and 2 gram dimethylbenzene, n-butanol mixed solvent is under whipped state, hybrid reaction 20 minutes, add 0.4 gram dispersion agent EFKA4010,0.4 gram dispersion agent DP9100 and 5 gram dimethylbenzene, n-butanol mixed solvent, after stirring, with ultrasonication 30 minutes, add 0.2 gram EFKA4009,0.2 gram EFKA2022,11 gram Resins, epoxy E-20 high-speed stirring 20 minutes, mix, carbon mitron/Resins, epoxy mixed system according to above-mentioned technology formation, carbon nanotube disperses easily, disperses evenly especially, and system is stablized.
Claims (5)
1, a kind of surface modification of carbon nanotube and the dispersing method in Resins, epoxy thereof, it is characterized in that: this method may further comprise the steps:
(a) be purified caliber 0.5-500nm, length is that 1-2 part carbon nanotube and the 1-2 part coupling agent of 200nm-40 μ m stirs hybrid reaction 10-20 minute in organic solvent;
(b) will add dispersion agent of 3-6 part and the organic solvent of 30-40 part in the above-mentioned mixture that mixes, after stirring, use ultrasonication 20-40 minute;
(c) with the Resins, epoxy high-speed stirring of above-mentioned finely dispersed solution and 55-60 part 10-20 minute, mix; Above-mentioned umber is weight part.
2, a kind of surface modification of carbon nanotube according to claim 1 and the dispersing method in Resins, epoxy thereof is characterized in that: Resins, epoxy is selected from least a among Resins, epoxy E-20, epoxy resin E-44 or the Resins, epoxy E-12.
3, a kind of surface modification of carbon nanotube according to claim 1 and the dispersing method in Resins, epoxy thereof is characterized in that: coupling agent is at least a in silane coupling agent or the titanate coupling agent.
4, a kind of surface modification of carbon nanotube according to claim 1 and the dispersing method in Resins, epoxy thereof is characterized in that: dispersion agent is at least a in polyacrylic ester or the modified polyurethane.
5, a kind of surface modification of carbon nanotube according to claim 1 and the dispersing method in Resins, epoxy thereof is characterized in that: organic solvent is selected from least a in dimethylbenzene, propyl carbinol or the pimelinketone.
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| CNB2005100097690A CN1295275C (en) | 2005-02-22 | 2005-02-22 | Method for surface modification of carbon nanotube and its dispersion method in epoxy resin |
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| CN1295275C true CN1295275C (en) | 2007-01-17 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100586843C (en) * | 2006-07-18 | 2010-02-03 | 中国科学院化学研究所 | Polymer inarching carbon nano-tube and method of manufacturing the same |
| TWI413613B (en) * | 2010-05-14 | 2013-11-01 | Taiwan Textile Res Inst | Carbon nanotube composite and method for preparing the same |
| CN101817971B (en) * | 2010-05-27 | 2012-01-11 | 哈尔滨工业大学 | Carbon micro-tube epoxy resin wave-absorbing composite material and preparation method thereof |
| CN102208622B (en) * | 2011-04-21 | 2013-03-20 | 湖南大学 | Method for preparing linear nano carbon conductive agent coated lithium iron phosphate anode material |
| CN102212322A (en) * | 2011-05-11 | 2011-10-12 | 烟台德邦科技有限公司 | Carbon nano tube reinforcing epoxy structural adhesive and method for preparing same |
| CN105820508A (en) * | 2016-04-25 | 2016-08-03 | 东莞市联洲知识产权运营管理有限公司 | Novel modified multi-walled carbon nanotube-epoxy resin composite material and preparation method thereof |
| CN105860141A (en) * | 2016-04-26 | 2016-08-17 | 深圳市博赛新材有限公司 | Method for carrying out modification treatment on heat conducting powder fillers and heat conducting fillers |
| CN105907042B (en) * | 2016-06-17 | 2018-06-22 | 华南理工大学 | A kind of functionalized carbon nano-tube epoxy resin nano composites and preparation method thereof |
| CN115558329A (en) * | 2022-11-03 | 2023-01-03 | 南京南大波平电子信息有限公司 | Method for dispersing carbon nano-tubes in wave-absorbing coating system and wave-absorbing coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410454A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite material and its in situ mass polymerization |
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1410454A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite material and its in situ mass polymerization |
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
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